CN108159002B - Preparation method of onion bionic multilayer structure controlled drug release carrier - Google Patents
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Abstract
The invention belongs to the technical field of soft material materials and pharmaceutical preparations, and provides a preparation method of an onion bionic multilayer structure controlled release carrier. And (3) dropwise adding the mixed solution A obtained by mixing and stirring the medicine and the chitosan solution into the mixed solution B of sodium hyaluronate and sodium tripolyphosphate, and stirring and curing to obtain single-layer medicine carrying gel balls with uniform particle size. And mixing the single-layer liquid medicine-carrying gel balls into the mixed solution A and the mixed solution B, stirring and curing to obtain two layers of liquid medicine-carrying gel balls with uniform particle sizes, and repeating the steps to obtain the multilayer hydrogel balls. The raw materials of the invention have biocompatibility, the preparation method is simple, and the multilayer drug-loaded gel sphere can be prepared in a large scale at one time, and has pH sensitivity; the purpose of controlling the drug release is achieved by controlling the layer number of the hydrogel spheres, the burst release of the drug can be avoided, and the administration times and the side effects of the drug can be reduced.
Description
Technical Field
The invention belongs to the technical field of soft material materials and pharmaceutical preparations, and relates to a preparation method of an onion bionic multilayer structure controlled release hydrogel carrier.
Background
Controlled drug release has a number of unique advantages over traditional drug delivery vehicle systems. Including local delivery of the drug to specific parts of the body, drug stability, reduced need for follow-up care and optimized drug absorption. Based on the above characteristics, hydrogels have been widely studied as carriers for controlled release drugs. Hydrogel drug delivery systems can be designed to exhibit a response to physical (e.g., temperature, light, electrical signals, and magnetic fields) or chemical (e.g., redox potential, glucose, specific ions, and pH) stimuli. Among different stimuli-sensitive hydrogels, because the pH of the internal environment of the human body varies significantly, for example, the pH of the stomach is low, the stomach is in an acidic environment, the pH of the intestinal tract is high, and the environment is close to neutral, the pH-sensitive hydrogel is often used as a carrier to realize the controlled release of the drug.
In the aspect of raw materials of the pH sensitive hydrogel, natural polymer materials are widely researched due to the characteristics of no toxicity, good biocompatibility and the like, but the problems of too fast release, burst release and the like of the drug in an environment with stronger acidity can occur, and the purpose of controlling the release of the drug cannot be achieved. Therefore, how to solve these problems and use non-toxic natural polymer materials becomes critical. The structure of the natural material is always a inspiration source, the bionic function can endow the material with excellent performance, and the onion outer skin forms 2-3 layers of membranous fresh scales, has the characteristics of air impermeability and water impermeability and is a good protective tissue of the onion. Therefore, the hydrogel is designed to have a compact multi-layer structure, the multi-layer compact structure can enable the medicine to be released layer by layer, and the release time is longer when the number of layers is larger. The number of layers of the hydrogel is designed according to the requirement of the drug on the release time, so that the problems of over-quick release and burst release of the drug are solved. In the invention, the aim of controlling the release of the medicament is achieved by preparing pH-sensitive 'onion' multi-layer structure hydrogel spheres and encapsulating the medicament in the hydrogel spheres.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of an onion bionic multilayer structure controlled release carrier. The preparation method can be used for preparing the multi-layer hydrogel sphere carrier with good biocompatibility and pH sensitivity, is simple, and can be used for large-scale preparation at one time. The hydrogel sphere drug carrier prepared by the method achieves the purpose of controlling drug release by controlling the number of layers of hydrogel spheres, can avoid burst release of drugs, and reduces the frequency of drug administration and drug side effects.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of an onion bionic multilayer structure controlled release carrier comprises the following steps:
first, a mixed solution A of a drug and a chitosan solution is prepared
1.1) dissolving chitosan powder in an acid solution with the concentration of 0.5-5%, and magnetically stirring at room temperature until chitosan is completely dissolved to obtain a chitosan solution with the concentration of 5-35 mg/mL. The acid solution comprises one or a mixture of more than two of dilute hydrochloric acid, acetic acid, pyruvic acid, phosphoric acid and propionic acid.
1.2) dispersing the medicine in the chitosan solution obtained in the step 1.1), magnetically stirring to uniformly mix the medicine and the chitosan solution, and performing vacuum defoaming until the medicine is completely defoamed to obtain a mixed solution A, wherein the medicine concentration in the mixed solution A is 0.05-0.7 mg/mL. The medicine comprises one of daunorubicin, adriamycin, curcumin, rifampicin, ranitidine, furazolidone and mecobalamin.
Secondly, preparing a mixed solution B of sodium hyaluronate and sodium tripolyphosphate
2.1) dissolving the sodium hyaluronate powder in deionized water, stirring the solution at room temperature until the solution is transparent, and defoaming the solution in vacuum until the solution is completely defoamed to obtain a sodium hyaluronate solution with the concentration of 0.5-20 mg/mL.
2.2) dissolving the sodium tripolyphosphate particles in deionized water, and magnetically stirring for 30 minutes to obtain a sodium tripolyphosphate solution with the concentration of 0.1-15 mg/mL.
2.3) mixing the sodium hyaluronate solution obtained in the step 2.1) with the sodium tripolyphosphate solution obtained in the step 2.2) according to the volume ratio of 1: 1-8, magnetically stirring uniformly, and defoaming in vacuum to obtain a mixed solution B.
Thirdly, preparing a multilayer hydrogel sphere
3.1) dropwise adding the mixed solution A into the mixed solution B, stirring, curing for 20-90 minutes at room temperature, and washing with deionized water to obtain single-layer liquid medicine carrying gel spheres with uniform particle sizes.
3.2) adding the single-layer liquid medicine carrying gel balls obtained in the step 3.1) into the mixed solution A, stirring, dripping the mixed solution A mixed with the hydrogel balls into the mixed solution B by using a dropper, stirring, curing for 20-90 minutes at room temperature, and washing by using deionized water to obtain the two-layer liquid medicine carrying gel balls with uniform particle sizes. The procedure is repeated to prepare a plurality of layers of hydrogel-loaded spheres. The prepared multilayer pH sensitive hydrogel sphere is a drug carrier with controllable drug release.
The prepared multilayer pH-sensitive hydrogel spheres were divided into three equal parts, which were placed in buffers of pH 1.2, pH 4.0 and pH7.4, respectively, and their release was observed, samples were taken at regular intervals, and the same amount of buffer was added at the same time as the sampling. This experiment was repeated three times. And measuring the light absorption value of the sample by using an ultraviolet spectrophotometer (Lambda 750s), and calculating by contrasting a standard curve to obtain the drug release amount.
Compared with the prior art, the invention has the beneficial effects that:
the onion bionic multilayer structure controlled-release liquid medicine gel ball prepared by the invention has pH sensitivity, and the accumulative release rates in buffer solutions with pH 1.2, pH 4.0 and pH7.4 for 12 hours can respectively reach 100%, 83.5% and 6.1%. Meanwhile, no burst release phenomenon exists at the beginning of release, and the number of hydrogel sphere layers can be prepared according to the drug release requirement. The method has the advantages of mild reaction conditions, simple requirements on instruments and equipment, simple and controllable preparation process and easy scale production; meanwhile, the purpose of controlling the release of the medicament can be achieved by controlling the layer number of the hydrogel spheres, the burst release of the medicament is avoided, and the administration times and the side effects of the medicament are reduced; the drug carrier material is a degradable biological material, has high biocompatibility and has wide market prospect in the aspect of drug loading.
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FIG. 1 is a schematic view (SEM) of a three-layer hydrogel sphere according to the present invention. FIG. 1(a) is a topographical view of the whole; FIG. 1(b) is a half sectional view; FIG. 1(c) is a partially enlarged view;
FIG. 2 is a graph showing the release of hydrogel spheres with three-layer structure according to the present invention under different pH conditions with time.
Detailed Description
The following detailed description of the present invention is provided in connection with specific examples to assist in further understanding, and is not intended to limit the invention.
Example 1
The preparation method of the hydrogel ball with the three-layer structure comprises the following steps:
dissolving chitosan in 2% acetic acid solution, stirring for 2 hours at room temperature by magnetic force until the solution is clear to obtain 20mL of chitosan solution with the concentration of 15mg/mL, adding 4mg of adriamycin, continuing stirring for 30 minutes until the solution is uniformly mixed, placing the solution in a vacuum drying oven for vacuum defoamation for 30 minutes, and removing bubbles in the solution to obtain a mixed solution A.
Dissolving sodium hyaluronate powder in deionized water, magnetically stirring at room temperature for 1 hour until the solution is transparent to obtain a sodium hyaluronate solution with the concentration of 20mg/mL, placing the sodium hyaluronate solution in a vacuum drying oven for vacuum defoaming for 30 minutes, and removing bubbles in the solution. The sodium tripolyphosphate was dissolved in deionized water and magnetically stirred at room temperature for 30 minutes to obtain 60mL of a 5mg/mL solution of sodium tripolyphosphate.
Mixing 20mL of 15mg/mL sodium hyaluronate solution with 60mL of 5mg/mL sodium tripolyphosphate solution, magnetically stirring uniformly, and defoaming in vacuum to obtain a mixed solution B.
And dropwise adding the mixed solution A into the mixed solution B, magnetically stirring and curing for 50 minutes, and washing with deionized water for 3 times to obtain the single-layer liquid medicine-carrying gel ball. And adding the obtained single-layer medicine-carrying hydrogel spheres into the mixed solution A, dripping the mixed solution A mixed with the hydrogel spheres into the mixed solution B by using a dropper, stirring, curing for 50 minutes at room temperature, and washing by using deionized water to obtain two layers of medicine-carrying hydrogel spheres. Repeating the steps to obtain three layers of the liquid medicine carrying gel balls.
Testing the drug release performance of the three-layer loaded hydrogel spheres:
the three-layer drug-loaded hydrogel spheres are equally divided into three parts, the three parts are respectively placed into buffer solutions with pH 1.2, pH 4.0 and pH7.4, the release conditions of the three parts are observed, samples are taken at intervals, and the same amount of buffer solution is added while the samples are taken.
And measuring the light absorption value of the sample by using an ultraviolet spectrophotometer (Lambda 750s), and calculating by contrasting a standard curve to obtain the drug release amount.
Example 2
The preparation method of the two-layer liquid medicine carrying gel ball comprises the following steps:
dissolving chitosan in 1% dilute hydrochloric acid solution, magnetically stirring for 2 hours at room temperature until the solution is clear to obtain 15mL of 5mg/mL chitosan solution, adding 5mL of curcumin solution (1.0mg/mL) dissolved in acetic acid, continuously stirring for 30 minutes until the solution is uniformly mixed, placing the mixture in a vacuum drying oven for vacuum defoamation for 30 minutes, and removing bubbles in the solution to obtain a mixed solution A.
Dissolving sodium hyaluronate powder in deionized water, magnetically stirring at room temperature for 1 hour until the solution is transparent to obtain a sodium hyaluronate solution with the concentration of 0.5mg/mL, placing the solution in a vacuum drying oven for vacuum defoaming for 30 minutes, and removing bubbles in the solution. The sodium tripolyphosphate is dissolved in deionized water, and the solution is magnetically stirred for 30 minutes at room temperature to obtain a sodium tripolyphosphate solution with the concentration of 1 mg/mL.
Mixing 10mL of 0.5mg/mL sodium hyaluronate solution with 20mL of 1mg/mL sodium tripolyphosphate solution, uniformly stirring by magnetic force, and defoaming in vacuum to obtain a mixed solution B.
And dropwise adding the mixed solution A into the mixed solution B, magnetically stirring and curing for 20 minutes, and washing with deionized water for 3 times to obtain the single-layer liquid medicine-carrying gel ball. And adding the obtained single-layer drug-loaded hydrogel spheres into the mixed solution A, dripping the mixed solution A mixed with the hydrogel spheres into the mixed solution B by using a dropper, stirring, curing for 20 minutes at room temperature, and washing by using deionized water to obtain two layers of hydrogel spheres.
Testing the drug release performance of the two-layer loaded hydrogel spheres:
the two layers of drug-loaded hydrogel spheres are equally divided into three parts, the three parts are respectively placed into buffer solutions with pH 1.2, pH 4.0 and pH7.4, samples are taken at intervals, and the same amount of buffer solution is added while the samples are taken.
And measuring the light absorption value of the sample by using an ultraviolet spectrophotometer (Lambda 750s), and calculating by contrasting a standard curve to obtain the drug release amount.
Example 3
The preparation method of the five-layer liquid medicine-carrying gel ball comprises the following steps:
dissolving chitosan in 0.5% phosphoric acid solution, magnetically stirring for 2 hours at room temperature until the solution is clear to obtain 25mL of 30mg/mL chitosan solution, adding 2mg of mecobalamin, continuously stirring for 30 minutes until the solution is uniformly mixed, placing the solution in a vacuum drying oven for vacuum defoamation for 30 minutes, and removing bubbles in the solution to obtain a mixed solution A.
Dissolving sodium hyaluronate powder in deionized water, magnetically stirring at room temperature for 1 hour until the solution is transparent to obtain a sodium hyaluronate solution with the concentration of 5mg/mL, placing the solution in a vacuum drying oven for vacuum defoaming for 30 minutes, and removing bubbles in the solution. The sodium tripolyphosphate is dissolved in deionized water, and the solution is magnetically stirred for 30 minutes at room temperature to obtain a sodium tripolyphosphate solution with the concentration of 15 mg/mL.
Mixing 25mL of 5mg/mL sodium hyaluronate solution with 25mL of 15mg/mL sodium tripolyphosphate solution, magnetically stirring uniformly, and defoaming in vacuum to obtain a mixed solution B.
And dropwise adding the mixed solution A into the mixed solution B, magnetically stirring and curing for 90 minutes, and washing with deionized water for 3 times to obtain the single-layer hydrogel spheres. And adding the obtained single-layer hydrogel spheres into the mixed solution A, dripping the mixed solution A mixed with the hydrogel spheres into the mixed solution B by using a dropper, stirring, curing for 90 minutes at room temperature, and washing by using deionized water to obtain two-layer hydrogel spheres. Repeating the above steps to obtain five layers of hydrogel-carrying balls.
Testing the drug release performance of the five-layer loaded liquid medicine gel balls:
equally dividing the five-layer drug-loaded hydrogel spheres into three parts, respectively placing the three parts into buffer solutions with pH 1.2, pH 4.0 and pH7.4, sampling at intervals, and adding the same amount of buffer solution while sampling.
And measuring the light absorption value of the sample by using an ultraviolet spectrophotometer (Lambda 750s), and calculating by contrasting a standard curve to obtain the drug release amount.
Claims (8)
1. A preparation method of an onion bionic multilayer structure controlled release carrier is characterized by comprising the following steps:
first, a mixed solution A of a drug and a chitosan solution is prepared
1.1) dissolving chitosan powder in an acid solution, and magnetically stirring at room temperature until chitosan is completely dissolved to obtain a chitosan solution;
1.2) dispersing the medicine in the chitosan solution obtained in the step 1.1), magnetically stirring to uniformly mix the medicine, and carrying out vacuum defoaming until the medicine is completely defoamed to obtain a mixed solution A, wherein the medicine concentration in the mixed solution A is 0.05-0.7 mg/mL;
secondly, preparing a mixed solution B of sodium hyaluronate and sodium tripolyphosphate
2.1) dissolving sodium hyaluronate powder in deionized water, stirring at room temperature until the solution is transparent, and defoaming in vacuum until the solution is completely defoamed to obtain a sodium hyaluronate solution with the concentration of 0.5-20 mg/mL;
2.2) dissolving the sodium tripolyphosphate particles in deionized water, and magnetically stirring for 30 minutes to obtain a sodium tripolyphosphate solution with the concentration of 0.1-15 mg/mL;
2.3) mixing the sodium hyaluronate solution obtained in the step 2.1) with the sodium tripolyphosphate solution obtained in the step 2.2) according to the volume ratio of 1: 1-8, magnetically stirring uniformly, and defoaming in vacuum to obtain a mixed solution B;
thirdly, preparing a multilayer hydrogel sphere
3.1) dropwise adding the mixed solution A into the mixed solution B, stirring, curing for 20-90 minutes at room temperature, and washing with deionized water to obtain single-layer liquid medicine carrying gel spheres with uniform particle sizes;
3.2) adding the single-layer liquid medicine carrying gel balls obtained in the step 3.1) into the mixed solution A, stirring, dripping the mixed solution A mixed with the hydrogel balls into the mixed solution B by using a dropper, stirring, curing for 20-90 minutes at room temperature, and washing by using deionized water to obtain two layers of liquid medicine carrying gel balls with uniform particle sizes; the multilayer loaded hydrogel spheres prepared by repeating the steps are multilayer pH sensitive hydrogel spheres, namely the drug carrier capable of controllably releasing the drug.
2. The method for preparing the onion biomimetic multilayer structure controlled release carrier according to claim 1, wherein the concentration of the acidic solution is 0.5-5%.
3. The method for preparing an onion biomimetic multilayer structure carrier with controlled release of drugs according to claim 1 or 2, characterized in that the acidic solution comprises one or a mixture of two or more of diluted hydrochloric acid, acetic acid, pyruvic acid, phosphoric acid, propionic acid.
4. The preparation method of the onion biomimetic multilayer structure controlled release carrier according to claim 1 or 2, wherein the concentration of the chitosan solution is 5-35 mg/mL.
5. The preparation method of the onion biomimetic multilayer structure controlled release carrier according to claim 3, wherein the concentration of the chitosan solution is 5-35 mg/mL.
6. The method for preparing the onion biomimetic multilayer structure carrier with controlled release of drugs according to claim 1, 2 or 5, characterized in that the drug comprises one of daunorubicin, doxorubicin, curcumin, rifampicin, ranitidine, furazolidone and mecobalamin.
7. The method for preparing an onion biomimetic multilayer structure controlled release carrier as claimed in claim 3, wherein the drug includes one of daunorubicin, doxorubicin, curcumin, rifampicin, ranitidine, furazolidone, and mecobalamin.
8. The method for preparing an onion biomimetic multilayer structure controlled release carrier as claimed in claim 4, wherein the drug includes one of daunorubicin, doxorubicin, curcumin, rifampicin, ranitidine, furazolidone, and mecobalamin.
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| IT1243390B (en) * | 1990-11-22 | 1994-06-10 | Vectorpharma Int | PHARMACEUTICAL COMPOSITIONS IN THE FORM OF PARTICLES SUITABLE FOR THE CONTROLLED RELEASE OF PHARMACOLOGICALLY ACTIVE SUBSTANCES AND PROCEDURE FOR THEIR PREPARATION. |
| EP1903982A4 (en) * | 2005-07-21 | 2011-03-16 | Fmc Biopolymer As | Medical devices coated with a fast dissolving biocompatible coating |
| KR100718329B1 (en) * | 2005-09-08 | 2007-05-14 | 광주과학기술원 | Polysaccharide-functionalized nanoparticle, drug delivery system for controlled release, and method of preparing the same |
| BRPI1005312A2 (en) * | 2009-01-30 | 2015-09-01 | Unilever Nv | Stable emulsion, process for the manufacture of an emulsion and product selected from the group consisting of a food product, a home care product, a personal care product and a pharmaceutical product. |
| CN102391537B (en) * | 2011-07-15 | 2013-06-05 | 厦门大学 | Multilayer aquagel, and preparation method and application thereof |
| CN103789813A (en) * | 2014-01-24 | 2014-05-14 | 北京化工大学常州先进材料研究院 | Method for preparing chitosan/hyaluronic acid layered composite membrane by utilizing electrophoretic deposition |
| CN106693078A (en) * | 2016-11-24 | 2017-05-24 | 西南交通大学 | Preparation method of drug-loaded layer-by-layer self-assembly coating |
| CN107412779B (en) * | 2017-04-17 | 2020-08-14 | 大连理工大学 | Preparation method of antitumor drug carrier with physical targeting |
| CN107281159B (en) * | 2017-06-29 | 2019-12-20 | 安徽大学 | Preparation method of sustained-release drug-loaded microcapsule with multilayer core-shell structure |
| CN107375995A (en) * | 2017-07-21 | 2017-11-24 | 临沂市人民医院 | A kind of preparation method based on layer assembly function selfreparing aquogel type dressing materials |
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